A kind of synthetic method of 4,4'-diaminodiphenyl ether

A technology of diaminodiphenyl ether and a synthesis method, which is applied in the field of synthesis of fine chemical intermediates, can solve the problems of large environmental pollution, strong corrosion, and many three wastes, and achieves the reduction of three wastes, the total cost, and the amount of hydrogen. Effect

Active Publication Date: 2021-03-16
青岛伯川特聚科技有限公司
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Problems solved by technology

Method ② more by-products and lower yield
Strong corrosiveness and great environmental pollution
Routes ③ and ④ are two routes commonly used in industrial production at present, but these two routes have higher requirements on equipment. To synthesize nitro compounds, concentrated sulfuric acid is used as a solvent, and the dosage is large. After the reaction, a large amount of water needs to be added for dilution. The target product is separated and a large amount of strongly acidic wastewater is produced, and there are many three wastes

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  • A kind of synthetic method of 4,4'-diaminodiphenyl ether
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  • A kind of synthetic method of 4,4'-diaminodiphenyl ether

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Embodiment Construction

[0024] The technical solutions in the embodiments of the present invention will be clearly and completely described below.

[0025] The present invention provides a kind of synthetic method of 4,4'-diaminodiphenyl ether, specific examples are as follows:

[0026] 1) Nitrosation reaction

[0027]

[0028] Weigh 72.4g (1.05mol) of sodium nitrite and dissolve it in 240ml of water, add 85g of diphenyl ether (0.5mol) into a 1L reaction vessel, slowly add the prepared sodium nitrite aqueous solution into the reaction vessel, start stirring, and control Temperature 0-5°C, slowly add 115g (1.1mol) of 35% concentrated hydrochloric acid dropwise, keep 0-5°C to continue the reaction for 1-1.5h after dropping, crystals are precipitated, filtered, and dried in vacuum at low temperature to obtain light yellow needle-shaped crystals 99.4 g, yield 87.1%.

[0029] Intermediate 4,4'-Dinitrosodiphenyl ether data analysis, see figure 1 .

[0030] Elemental Analysis C 12 h 8 N 2 o 3 , T...

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Abstract

The invention discloses a synthetic method of 4, 4'-diaminodiphenyl ether. The synthetic method comprises the following steps: S1, nitrosation reaction: adding sodium nitrite and diphenyl ether into awater phase, slowly dropwise adding hydrochloric acid in a range of 0-5 DEG C till the reaction is finished, separating out crystals, filtering the crystals, and drying the crystals in vacuum to obtain 4, 4'-diaminodiphenyl ether, wherein the reaction process is as follows; and S2, reductive reaction: adding the obtained solid into a high pressure kettle, adding a catalyst by taking alcohol as asolvent, pressurizing hydrogen to 0.5-4 MPa, heating and stirring the mixture to 70-120 DEG C, and keeping the temperature for 2-6 hours to obtain 4, 4'-diaminodiphenyl ether. The synthetic method disclosed by the invention can reduce the production cost, reduce the environmental pollution, improve the safety coefficient and reduce the emission of three wastes.

Description

technical field [0001] The invention relates to the synthesis of fine chemical intermediates, in particular to a synthesis method of 4,4'-diaminodiphenyl ether. Background technique [0002] ODA (4,4'-diaminodiphenyl ether) is an important fine chemical intermediate, mainly used as a raw material for the production of polyimide resin, polyamide resin, epoxy resin and other products, while 4,4 '-Diaminodiphenyl ether can also be used as a cross-linking agent, and can also be used to replace carcinogenic benzidine to produce azo dyes and reactive dyes. [0003] At present, there are mainly four routes for the synthesis of ODA, namely: ① p-dinitrobenzene method, ② diphenyl ether nitration method, ③ p-nitrochlorobenzene and p-nitrophenol condensation method, ④ p-nitrochlorobenzene one-step condensation method legitimate. The raw materials in method ① are volatile and highly toxic, and cause great environmental hazards. Method ② The by-products are abundant and the yield is lo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/02C07C217/90
CPCC07C201/00C07C213/02C07C207/04C07C217/90
Inventor 陈晨武金波谭立春丁玉
Owner 青岛伯川特聚科技有限公司
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